4354-73-8 2-亚环己基丙二腈
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安全说明
运输信息:常温运输。危险描述:非危险化学品。
用途与制备
化学合成。
化学合成
产率:100% 合成条件:at 25℃; for 2 h; 实验步骤:相应的反应(a)至(p)是通过在搅拌下和在5ml溶剂(二甲基甲酰胺(己烷)DMF或乙腈(MeCN))中,1毫摩尔羰基化合物和1毫摩尔活化甲醇的反应实现的。 在实施例1中制备0.0035g'HDT-F'催化剂。在每种情况下,通过在板上进行色谱法跟踪反应进程。 在反应结束时,过滤催化剂,滤液用水洗涤,产物用硫酸钠萃取并在低压下浓缩。 基于在最终培养基中观察到的NMR光谱,基于反应过程中消耗的R1R2CO酮化合物计算所示产率。 参考文献:[1] Patent: US2005/250963, 2005, A1. Location in patent: Page/Page column 5 [2] Green Chemistry, 2010, vol. 12, # 3, p. 514 - 517 [3] Synlett, 2000, # 7, p. 1016 - 1018 [4] Collection of Czechoslovak Chemical Communications, 2005, vol. 70, # 10, p. 1727 - 1736 [5] European Journal of Organic Chemistry, 2008, # 28, p. 4763 - 4768 [6] RSC Advances, 2013, vol. 3, # 45, p. 23075 - 23079 [7] Russian Chemical Bulletin, 2013, vol. 62, # 3, p. 683 - 686 [8] Izv. Akad. Nauk, Ser. 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Chem., 2016, vol. 128, p. 9206 - 9210,5 [82] Monatshefte fur Chemie, 2016, vol. 147, # 7, p. 1243 - 1249 [83] Molecules, 2016, vol. 21, # 12, [84] Polymer, 2017, vol. 112, p. 342 - 350 [85] Molecular Catalysis, 2018, vol. 453, p. 93 - 99 [86] Green Chemistry, 2018, vol. 20, # 23, p. 5336 - 5345 以环己酮和丙二腈为原料合成2-环己基亚己基丙二腈的一般步骤如下:在搅拌条件下,将1毫摩尔环己酮(羰基化合物)和1毫摩尔丙二腈(活化甲醇)溶于5毫升溶剂(二甲基甲酰胺(DMF)或乙腈(MeCN))中。加入0.0035克'HDT-F'催化剂(如实施例1所述制备)。反应进程通过薄层色谱法(TLC)监测。反应完成后,过滤去除催化剂,滤液用水洗涤,产物用硫酸钠干燥后,在减压条件下浓缩。产率基于反应过程中消耗的环己酮量,通过核磁共振(NMR)光谱分析最终产物确定。 参考文献:[1] Patent: US2005/250963, 2005, A1. Location in patent: Page/Page column 5 [2] Green Chemistry, 2010, vol. 12, # 3, p. 514 - 517 [3] Synlett, 2000, # 7, p. 1016 - 1018 [4] Collection of Czechoslovak Chemical Communications, 2005, vol. 70, # 10, p. 1727 - 1736 [5] European Journal of Organic Chemistry, 2008, # 28, p. 4763 - 4768